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CN103059569A - Cation silicone emulsion capable of rapidly breaking emulsion, preparing method and application thereof - Google Patents

Cation silicone emulsion capable of rapidly breaking emulsion, preparing method and application thereof Download PDF

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CN103059569A
CN103059569A CN2012105711655A CN201210571165A CN103059569A CN 103059569 A CN103059569 A CN 103059569A CN 2012105711655 A CN2012105711655 A CN 2012105711655A CN 201210571165 A CN201210571165 A CN 201210571165A CN 103059569 A CN103059569 A CN 103059569A
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silicone oil
cation
emulsion
polydimethylsiloxane
emulsified silicone
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CN103059569B (en
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张磊
杨利超
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DAQIAN HI-NEW TECH RESEARCH CENTER Co Ltd SHANTOU CITY
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DAQIAN HI-NEW TECH RESEARCH CENTER Co Ltd SHANTOU CITY
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Abstract

The invention provides cation silicone emulsion capable of rapidly breaking emulsion during the usage process to improve the silicone oil usage efficiency. The cation silicone emulsion includes by weight 25-70% of poly-dimethyl siloxane, 2-20% of poly- quaternary ammonium salt, 2-15% of macromolecule emulgator and remaining deionized water, and the cation silicone emulsion is formed by emulsification. The macromolecule emulgator is a macromolecule cationic opsonizing emulgator H305. The cation silicone emulsion can exist in a liquid shampoo system; achieve the effect of rapid breaking emulsion when the cation silicone emulsion is used. When the cation silicone emulsion is added into the liquid shampoo system to be used as an opsonizing component, the cation silicone emulsion can break the emulsion rapidly under the dilution of a little water, on one hand, the poly-dimethyl siloxane can be deposited on the surface of the hair to the uttermost so that the effects of smoothness in wet hair, brightness and no greasiness in dry hair can be achieved. On the other hand, the addition quantity of the silicone emulsion is reduced; the cost of the liquid shampoo is saved. The invention further provides the preparing method of the cation silicone emulsion and the application for the opsonizing component in the liquid shampoo system.

Description

A kind of cation emulsified silicone oil that can fast emulsion breaking and its preparation method and application
Technical field
The present invention relates to a kind of silicone oil, relate in particular to a kind of silicone emulsion, more specifically relate to a kind of cation emulsified silicone oil that in use can fast emulsion breaking uses effect to improve silicone oil.The invention still further relates to preparation method and the application in the shampoo system of this cation emulsified silicone oil.
Background technology
Silicone oil is being commonly called as of linear polysiloxanes product, and normally used silicone oil, organic group are methyl all, therefore be called methyl-silicone oil or dimethyl siloxane or polydimethylsiloxane; The polymerization degree or the state under the normal temperature according to methyl-silicone oil are different, (general viscosity is in 10000 centistokes also can be divided into silicone oil with low viscosity, also be that the polymerization degree is lower), (general viscosity is between 10000 centistokes and 100,000 centistokes for viscous silicone fluid, also be that the polymerization degree is medium) and silicone grease (general viscosity surpasses 100,000 centistokes, also is that the polymerization degree is higher).
Polydimethylsiloxane is owing to can make hair have unique soft feel(ing) and high resilience, that component is added in a kind of conditioning the most frequently used in the shampoo, yet polydimethylsiloxane has water-fast characteristic, if directly add in the shampoo, in appearance, can cause the phenomenons such as shampoo is thinning, layering to occur, simultaneously on dispersiveness, also there is difficulties in dispersion, disperses the problems such as inhomogeneous, therefore polydimethylsiloxane can not directly add in the shampoo and uses, but with after the polydimethylsiloxane emulsification, join in the shampoo again.During use, take a morsel (general 5 gram in) contain the shampoo of silicone emulsion after hair surface is rubbed, use again flushing with clean water, at this moment, after a small amount of shampoo ran in a large number the clear water dilution of (generally being more than 500 grams), silicone emulsion began breakdown of emulsion, and polydimethylsiloxane is deposited on the surface of hair gradually, form the molsink lamination, reach sliding effect suitable, light and non-greasy when doing when making hair wet.
The use of silicone emulsion in the shampoo system reached time more than ten years, but the silicone emulsion of selling on the market at present, the emulsifying agent that adopts all is a little small-molecular emulsifiers, such as isomerous tridecanol ether, lauryl alcohol sulfuric ester sodium salt, palmityl trimethyl ammonium chloride, octadecyl trimethyl ammonium chloride, laureth etc., these small-molecular emulsifiers are very good to the firmness of polydimethylsiloxane emulsification parcel, the emulsifying effectiveness quite stable, but these silicone emulsions also are not easy breakdown of emulsion in the hair washing process, a large amount of clear water dilution ability breakdowns of emulsion need to be arranged, if extension rate is inadequate, most silicone emulsion is toward contact be not able to do in time breakdown of emulsion and deposition, just directly washed out by clear water, only have seldom a part of silicone oil can be deposited on the hair surface, play the effect of nursing, cause the usefulness of silicone oil to can not get fully playing so on the one hand, the appearance of the problems such as the high expensive of shampoo also causes the waste of silicone emulsion or clear water on the other hand.
Summary of the invention
Thereby the purpose of this invention is to provide a kind of cation emulsified silicone oil that silicone oil uses effect that in use can fast emulsion breaking improves.
For realizing above purpose, cation emulsified silicone oil that can fast emulsion breaking of the present invention, by comprising that components by weight percent is that polydimethylsiloxane 25-70%, polyquaternium 2-20%, macromolecule emulsifier 2%-15% and surplus deionized water form through emulsification, the preferred macromolecule cation conditioning of macromolecule emulsifier emulsifying agent H305.
Macromolecule cation conditioning emulsifying agent H305 is that the present patent application people produces and has the macromolecule emulsifier that the market can buy now, and it is to be obtained with reversed emulsion polymerization by polymethyl acyl-oxygen ethyl-trimethyl salmiac, C13-16 isoparaffin, tridecyl alcohol polyethers-6 and hydromining.
Consider that polydimethylsiloxane dispersion problem and the polydimethylsiloxane of different viscosity in process of production has unique effect separately, above-mentioned polydimethylsiloxane is that viscosity is that polydimethylsiloxane and the viscosity of 1,000,000 centistokes is the mixture of the polydimethylsiloxane of 50 centistokes, and viscosity is the polydimethylsiloxane of 1,000,000 centistokes and the preferred 0.4-1 ︰ 1 of polydimethylsiloxane ratio that viscosity is 50 centistokes.
In order to make cation emulsified silicone oil when possessing good elimination antistatic property, also possess good flush performance, above-mentioned polyquaternium preferred polyquaternium-47 and polyquaternium-37, the preferred 1:1 of ratio of polyquaternium-47 and polyquaternium-37.
Polyquaternium-47 and polyquaternium-37 all is products that existing market can buy, the chemical name of polyquaternium-47 is N, N, N-trimethylammonium-3-[(2-methyl isophthalic acid-oxo-2-propenyl) amino]-1-the third ammonium muriate and 2-methyl acrylate and the acrylic acid polymkeric substance of 2-, the chemistry of polyquaternium-37 is called N, N, N-trimethylammonium-2-[(2-methyl isophthalic acid-oxygen-2-propenyl) oxygen base] homopolymer of ethylamine hydrochloride.
In order to prolong the quality guaranteed period of product, the feed composition of above-mentioned cation emulsified silicone oil also comprises the Kathon CG of 0.1-0.2%.
The present invention also provides a kind of preparation method of above-mentioned cation emulsified silicone oil that can fast emulsion breaking, and the method in turn includes the following steps:
(1) polydimethylsiloxane is added in the agitator kettle, stir and be warmed up to 50 ± 2 ℃;
(2) add successively polyquaternium, macromolecule emulsifier, at every turn reinforced complete all to stir after, add again another kind of raw material;
(3) add the deionized water of 60-65% amount, after stirring, with 3200-3500 rev/min speed homogeneous 10 minutes;
(4) add the deionized water of residual content, after stirring, with 3200-3500 rev/min speed homogeneous 10 minutes, blowing.
In order to control the particle diameter of silicone emulsion, in order to better improve the speed of silicone emulsion breakdown of emulsion and deposition, in the aforesaid method, the preferred 10-20 of stirring velocity of step (1) rev/min, the preferred 50-70 of stirring velocity of step (2) rev/min.
More stable in product shelf life in order to guarantee silicone emulsion, in the aforesaid method, the adding speed of step (3) and step (4) deionized water is 50-52KG/ hour.
In order to prolong the quality guaranteed period of product, in the aforesaid method, before the blowing of step (4), add 0.1-0.2 part Kathon CG, stir.
In order to guarantee that cation emulsified silicone oil has the homogeneity of better stability, size distribution, in the aforesaid method, the system temperature when step (3) and step (4) homogeneous should remain on 50 ± 2 ℃.
Above-mentioned can fast emulsion breaking cation emulsified silicone oil in the shampoo system as the application of conditioning component, the addition of cation emulsified silicone oil in the shampoo system is 3-3.5%.
The present invention can fast emulsion breaking cation emulsified silicone oil, adopt the positively charged ion polyquaternium to come polydimethylsiloxane is carried out surface treatment, make it have certain cationic characteristic, adopt again macromolecule emulsifier that polydimethylsiloxane is carried out emulsification, obtain wrapping up firmly suitable silicone emulsion, the existence that this silicone emulsion is can either be in the shampoo system stable can reach again the effect of fast emulsion breaking during use; In addition, the adding of positively charged ion polyquaternium also can reduce the usage quantity of cation opsonizing agent in the shampoo system, plays the effect that reduces cost.Cation emulsified silicone oil of the present invention, add in the shampoo system when using as conditioning component, can fast emulsion breaking under the dilution of a small amount of clear water, can make polydimethylsiloxane be deposited on to greatest extent the surface of hair on the one hand, reach sliding effect suitable, light and non-greasy when doing when making hair wet, also can reduce on the other hand the add-on of silicone emulsion, the cost of shampoo is minimized and the minimizing of the hourly water consumption of having one's hair wash.Conventional emulsifying process is adopted in the preparation of the sub-silicone emulsion of the present invention, by the control to temperature, stirring velocity and amount of water, reaches suitable parcel fastness.
Embodiment
The preparation of macromolecule cation conditioning emulsifying agent H305:
(1) 40 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides are mixed in 40 parts in water, for subsequent use:
(2) with in 12 parts of adding reactors of C13-16 isoparaffin, the control stirring velocity adds 2 parts of these Pan 83 of emulsifying agent at 40 rev/mins, stirs;
(3) the control stirring velocity slowly adds the prewired thing of step (1) at 60 rev/mins, and feed rate is controlled at 60 kg/hours, reinforced complete after, continue to stir 15 minutes;
(4) add 1 kilogram of 10% ammonium persulfate aqueous solution, stir;
(5) control temperature of reaction about 90 ℃ with water coolant and stirring velocity, reacted 5 hours;
(6) add 0.5 kilogram of 10% sodium sulfite aqueous solution, stir, make reaction terminating;
(7) add 8 parts tridecyl alcohol polyethers-6, stir, obtain polymer conditioning emulsifying agent H305.
Embodiment 1
1, prescription:
Polydimethylsiloxane (50 centistoke) 28.00 Kg
Polydimethylsiloxane (1,000,000 centistoke) 12.00 Kg
Polyquaternium-47 4.00 Kg
Polyquaternium-37 4.00 Kg
Macromolecule cation conditioning emulsifying agent H305 8.00 Kg
Kathon CG 0.15 Kg
Deionized water 43.85 Kg
2, preparation
(1) polydimethylsiloxane (50 centistoke) and polydimethylsiloxane (1,000,000 centistoke) are added in the agitator kettle, stir with 15 rev/mins speed and be warmed up to 50 ℃;
(2) add polyquaternium-47, polyquaternium-37, after stirring with 60 rev/mins stirring velocitys, add again macromolecule cation conditioning emulsifying agent, stir with 60 rev/mins stirring velocitys;
(3) with 50KG/ hour speed, add 25 kilograms of deionized waters, after stirring, keeping the temperature of system was 50 ℃, with 3200 rev/mins speed homogeneous 10 minutes;
(4) with 50KG/ hour speed, add the deionized water of residual content, after stirring, keeping the temperature of system was 50 ℃, with 3200 rev/mins speed homogeneous 10 minutes;
(5) add Kathon CG, rear blowing stirs.
The product fluid that is creamy white, viscosity is at 10000mPaS.
Embodiment 2
1, prescription
Polydimethylsiloxane (50 centistoke) 8.40 Kg
Polydimethylsiloxane (1,000,000 centistoke) 3.80 Kg
Polyquaternium-47 1.20 Kg
Polyquaternium-37 1.20 Kg
Macromolecule cation conditioning emulsifying agent H305 2.60 Kg
Kathon CG 0.05 Kg
Deionized water 12.75 Kg
2, preparation
(1) polydimethylsiloxane (50 centistoke) and polydimethylsiloxane (1,000,000 centistoke) are added in the agitator kettle, stir with 15 rev/mins speed and be warmed up to 50 ℃;
(2) add polyquaternium-47, polyquaternium-37, after stirring with 60 rev/mins stirring velocitys, add again macromolecule cation conditioning emulsifying agent, stir with 60 rev/mins stirring velocitys;
(3) with 50KG/ hour speed, add 7.65 kilograms of deionized waters, after stirring, keeping the temperature of system was 50 ℃, with 3200 rev/mins speed homogeneous 10 minutes;
(4) with 50KG/ hour speed, add the deionized water of residual content, after stirring, keeping the temperature of system was 50 ℃, with 3200 rev/mins speed homogeneous 10 minutes;
(5) add Kathon CG, rear blowing stirs.
The product fluid that is creamy white, viscosity is at 9000mPaS.
(2) Application Example
1, the product that above-described embodiment 1 or 2 is obtained adds in the shampoo of following prescription, and is as follows with the shampoo prescription that uses commercially available silicone emulsion:
Figure 2012105711655100002DEST_PATH_IMAGE001
Lauryl sulfate ester ammonium salt (70%) in the above-mentioned prescription refers to the lauryl sulfate ester ammonium salt of 70% content, and other therewith roughly the same; Commercially available silicone emulsion 1 is the DC-7137 silicone emulsion of Dow corning (Dow Corning) company, commercially available silicone emulsion 2 is Si Luoke silicone oil emulsions 2963 of Guangzhou Si Luoke chemistry company limited, the silicone emulsion SF-505 that commercially available silicone emulsion 3 is Guangdong Biaomei Silicon and Fluoride New Materials Co., Ltd..Use is added with the product of the prescription acquisition of the embodiment of the invention 1 or 2 positively charged ion silicone oil, light and non-greasy when cunning was suitable, dried when hair was wet.
2, shampoo manufacture craft
(1) will remain deionized water and add in the pot, and under agitation add cation guar gum (C-14S) and continued rapid stirring approximately 5 minutes;
(2) under rapid stirring, add cationic hydroxyethyl cellulose (JR-400), begin to heat up 70~75 ℃, stir after 5 minutes and to add the lemon aqueous acid and continue to stir 10 minutes, make its dissolving fully;
(3) under agitation add successively lauryl sulfate ester ammonium salt, lauryl alcohol sulfuric ester sodium salt, sodium lauroyl glutamate, cocoyl CAB, pearly-lustre dibasic acid esters, continue to be warming up to 70~75 ℃, dissolve complete;
(4) the material body all begins cooling after the dissolving evenly, and temperature is down to 50 ℃, adds silicone emulsion and stirs;
(5) temperature be down to below 45 ℃ add essence, Kathon CG stirs, and gets final product discharging.
3, de-emulsification speed test:
Under the condition of 25 ℃ of room temperatures, in 150 milliliters beaker, accurate weighing 5 grams, 4 grams, 3 grams, 2 grams, 1 restrain the above-mentioned product of respectively filling a prescription respectively, add 100 ml deionized water, under 60 rev/mins stirring velocity, stir after 1 minute, leave standstill, observe the material situation in the beaker, the result is as follows:
Figure 907192DEST_PATH_IMAGE002
By above-mentioned phenomenon as can be known, the shampoo silicone emulsion when diluting 20 times that is added with the cation emulsified silicone oil of the present invention just can reach breakdown of emulsion, and the shampoo that adds other commercially available silicone emulsions substantially all need to can reach breakdown of emulsion by silicone emulsion after diluting 50 times, this shows, the de-emulsification speed of the cation emulsified silicone oil of the present invention is far above similar commercially available prod.

Claims (10)

  1. One kind can fast emulsion breaking cation emulsified silicone oil, be by comprising that components by weight percent is that polydimethylsiloxane 25-70%, polyquaternium 2-20%, macromolecule emulsifier 2%-15% and the emulsification of surplus deionized water form, macromolecule emulsifier is macromolecule cation conditioning emulsifying agent H305.
  2. 2. cation emulsified silicone oil that can fast emulsion breaking according to claim 1, it is characterized in that: described polydimethylsiloxane is that viscosity is that polydimethylsiloxane and the viscosity of 1,000,000 centistokes is the mixture of the polydimethylsiloxane of 50 centistokes, and viscosity is the polydimethylsiloxane of 1,000,000 centistokes and the preferred 1 ︰ 0.4-1 of polydimethylsiloxane ratio that viscosity is 50 centistokes.
  3. 3. cation emulsified silicone oil that can fast emulsion breaking according to claim 1 and 2 is characterized in that: described polyquaternium preferred polyquaternium-47 and polyquaternium-37, the preferred 1:1 of ratio of polyquaternium-47 and polyquaternium-37.
  4. 4. cation emulsified silicone oil that can fast emulsion breaking according to claim 3, it is characterized in that: the feed composition of described cation emulsified silicone oil also comprises the Kathon CG of 0.1-0.2%.
  5. 5. the preparation method of a cation emulsified silicone oil that can fast emulsion breaking claimed in claim 1 in turn includes the following steps:
    (1) polydimethylsiloxane is added in the agitator kettle, stir and be warmed up to 50 ℃;
    (2) add successively polyquaternium, macromolecule emulsifier, at every turn reinforced complete all to stir after, add again another kind of raw material;
    (3) add the deionized water of 60-65% amount, after stirring, with 3200-3500 rev/min speed homogeneous 10 minutes;
    (4) add the deionized water of residual content, after stirring, with 3200-3500 rev/min speed homogeneous 10 minutes, blowing.
  6. 6. cation emulsified silicone oil that can fast emulsion breaking according to claim 5 is characterized in that: in the described method, and the preferred 10-20 of stirring velocity of step (1) rev/min, the preferred 50-70 of stirring velocity of step (2) rev/min.
  7. 7. cation emulsified silicone oil that can fast emulsion breaking according to claim 6, it is characterized in that: in the described method, the adding speed of step (3) and step (4) deionized water is 50-52KG/ hour.
  8. 8. cation emulsified silicone oil that can fast emulsion breaking according to claim 7 is characterized in that: in the described method, add 0.1-0.2 part Kathon CG before the blowing of step (4), stir.
  9. 9. cation emulsified silicone oil that can fast emulsion breaking according to claim 8, it is characterized in that: in the described method, the system temperature when step (3) and step (4) homogeneous remains on 50 ± 2 ℃.
  10. A claim 1-4 described can fast emulsion breaking cation emulsified silicone oil in the shampoo system as the application of conditioning component, the addition of cation emulsified silicone oil in the shampoo system is 3-3.5%.
CN201210571165.5A 2012-12-26 2012-12-26 Cation silicone emulsion capable of rapidly breaking emulsion, preparing method and application thereof Active CN103059569B (en)

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Publication number Priority date Publication date Assignee Title
CN112877112A (en) * 2021-01-15 2021-06-01 宋子云 Efficient lubricating oil demulsifier and production method thereof

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CN112877112A (en) * 2021-01-15 2021-06-01 宋子云 Efficient lubricating oil demulsifier and production method thereof

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